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1.
高效液相色谱法分离水田除草剂萘丙胺光学异构体   总被引:3,自引:0,他引:3  
施介华  徐秀珠 《分析化学》1999,27(12):1428-1430
采用高效液相色谱法分离水田除草剂萘丙胺光学异构体。实验结果表明,在键合(S)-(+)-N-(3,5-二硝基苯甲酰基)苯甘氨酸[3,5-DNB-(S)-(+)-PG]手性色谱柱上以正已烷/异丙醇(100/10,V/V)为流动相时,能较好地分离其萘丙胺的光学异构体,其容量因子分别为5.81和6.20;分离因子为1.08。  相似文献   

2.
制备手性色谱拆分氧氟沙星光学异构体   总被引:4,自引:1,他引:3  
曾苏  宗俭  潘莉  王似菊 《色谱》1996,14(4):280-281
 利用配合交换原理,采用手性流动相添加剂方法,在反相高效液相色谱(RP-HPLC)制备柱上,拆分了氧氟沙星的两种对映体。流动相组成为手性添加剂溶液(含6mmol/LL-苯丙氨酸和3mmol/LCuSO4)-CH3OH(84:16),流速4.6mL/min,紫外检测波长293nm。经提取纯化后,确证首先洗脱的是S-(+)-氧氟沙星,后一个洗脱的是R-(+)-氧氟沙星。经对映体选择性分析方法测定,制备获得的两种对映体的光学纯度均大于99%。  相似文献   

3.
以L-抗坏血酸(1)为原料, 经3 步反应制得(S)-缩异丙氧叉甘油醛(4). 该手性醛与苄胺缩合制得相应的手性亚胺(5). 甘氨酸经保护后制成酰氯, 在有机碱作用下首先生成不稳定的烯酮(8), 继与手性亚胺5 迅速进行[2+ 2]环加成反应, 合成标题化合物N-苄基-3(S)-邻苯二甲酰亚胺基-4(S)-[4(S)-2,2-二甲基-1,3-二氧环戊-4-基]-2-氧吖丁啶. 由于环加成的面向立体选择性容易控制, 由此所得产物的光学纯度和化学收率均较高  相似文献   

4.
二氯菊酯光学异构体的分析   总被引:3,自引:1,他引:2       下载免费PDF全文
利用顺式二氯菊酯和反式二氯菊酸的溶解度不同及pKa值的差异,分离二氯菊酸中的顺式体和反式体,可取得较好的效果(反式二氯菊酸收率83.7%,顺式二氯菊酸收率88.9%),以S(-)-α-甲基苄胺为拆分剂,对顺式-2,2-二甲基-3-3(2,2-二氯乙烯基)环丙烷羧酸酯(俗称顺式二氯菊酯)类杀虫剂合成中间体0顺式-2,2-二甲基-3-(2,2-二氯乙烯基)环丙烷羧酸(俗称顺式二氯菊酸)进行拆分,可以得到其旋光异构体;其旋光异构体与S(-)-α-甲基苄胺衍生化,生成相应的酰胺;经TLC纯化后,以外消旋顺式二氯菊酸酰胺作为对照,用HPLC检测其旋光异构体的光学纯度;结果显示,顺式-R(+)-2,2-二甲基-3-(2,2-二氯乙烯基)环丙烷羟酸光学纯度为93.7%,顺式-S(-)-2,2-二甲基-3-(2,2-二氯乙烯基)环丙烷羧酸光学纯度为81.8%,对反式二氯菊酸的光学纯度分析,可采用类似的方法:经顺,反分离,旋光异构体拆分获得的高效中间体,再进行后序合成,其顺反比,旋光纯度不变。  相似文献   

5.
赵军 《合成化学》1998,6(4):442-444
以光学活性L-乳酸为原料,经还原得(2S)-1,2-丙二醇(2),再经亚硫酰环化、亲核加成及酸解反应,得到手性合成子(3S)-β-羟基丁酸,收率58.4%(以的2计),光学纯度大于90%。  相似文献   

6.
在THF溶液中,40-60℃及0.3-0.5MPa氢压条件下,[RuCl2(cht)]2+(S)-BINAP手性催化剂体系催化不饱和手性缩酮2选择加氢,再经脱去手性二醇,即可高立体选择性地制得(R)-3-甲基环十五烷酮(4,(R)-(-)-麝香酮),化学收率≥95%,光学纯度≥97%.手性缩酮2由D-苏糖醇或D-葡萄糖衍生的手性二醇3与3-甲基环十五烯-2-酮1生成.  相似文献   

7.
高效液相色谱法测定灭尔痛片的组分含量   总被引:2,自引:2,他引:0  
采用高效液相色谱法同时测定灭尔痛片中对乙酰氨基酚、异丙基安替比林、及咖啡因3种成分的含量。色谱条件为:ODS柱,甲醇+水(60+40)为流动相,检测波长为254nm。方法线性范围分别为:24~120mg/L(r=09976);12~60mg/L(r=09994);4~20mg/L(r=09994)。各组分的平均回收率(n=6)分别为:1003%,RSD=042%;997%,RSD=069%;992%,RSD=046%。该法操作简便、快捷,结果准确。  相似文献   

8.
用高温固相法合成了系列化合物RE0.06La0.94M2O6Br(M=Nb,Ta;RE=Eu,Tb,Pr,Sm),并测定了其激发和发射光谱,室温下Eu3+、Tb3+、Pr3+、Sm3+在稀土-铌(钽)复合溴氧化物中呈现特征激发谱线,但Nb和Ta的光谱特性稍有不同.  相似文献   

9.
用2-乙基己基膦酸单2-乙基己酯萃取色谱分离-原子发射光谱测定超高纯Sm2O3、Eu2O3、Gd2O3中痕量稀土杂质,可用于纯度为999999%~9999999%(不含非稀土杂质)Sm2O3、Eu2O3、Gd2O3的纯度分析,14个稀土杂质的回收率在67%~133%之间,相对标准偏差±64%~±184%,分离周期10~14h。  相似文献   

10.
研究n-β(氨乙基)-γ(氨丙基)三乙氧基硅烷[NH2(CH2)2NH(CH2)3Si(OEt)3]与二甲基二乙氧基硅烷[(CH3)2Si(OEt)2]共水解,制备含-(CH2)3NH(CH2)2NH2功能基的聚硅氧烷配位体。用IR、1HNMR和元素分析法对共聚产物的结构进行了分析,同时用紫外-可见光谱法和SEM考察了共聚产物与Cu2+等金属离子的络合作用。结果发现,两种单体进行了共水解反应,而且随着NH2(CH2)2NH(CH2)3Si(OEt)3比例增加,水解程度提高。共聚产物可以与Cu2+离子形成稳定的络合物,但不能与Zn2+离子或Al3+离子形成稳定的络合物或螯合物。  相似文献   

11.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

12.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.  相似文献   

13.
The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.  相似文献   

14.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

15.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

16.
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.  相似文献   

17.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion.  相似文献   

18.
19.
An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.  相似文献   

20.
Quercetin, the polyphenolic compound, which has the highest daily intake, is well known for its protective effects against aging diseases and has received a lot of attention for this reason. Both quercetin 3-O-β-d-glucuronide and quercetin 3′-O-β-d-glucuronide are human metabolites, which, together with their regioisomers, are required for biological as well as physical chemistry studies. We present here a novel synthetic route based on the sequential and selective protections of the hydroxyl functions of quercetin allowing selective glycosylation, followed by TEMPO-mediated oxidation to the glucuronide. This methodology enabled us to synthesize the five O-β-d-glucosides and four O-β-d-glucuronides of quercetin, including the major human metabolite, quercetin 3-O-β-d-glucuronide.  相似文献   

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